JP6021828B2 - System and method for cooling a chromatography pump head - Google Patents

Description

  This application claims priority from US Provisional Patent Application No. 61 / 451,209, filed March 10, 2011. The entire contents of US Provisional Patent Application No. 61 / 451,209 are incorporated herein by reference.

  The present invention relates generally to actuators. In particular, the present invention relates to a system and method for cooling the pump head of an actuator.

  Supercritical fluid chromatography (SFC) generally uses a highly compressible mobile phase that utilizes carbon dioxide (CO2) as the main component. The pump is cooled to a temperature below the critical temperature to ensure that this component remains in the liquid.

  In one aspect, the invention features an actuator that includes a support plate and a pump head secured to one side of the support plate. The pump head is in thermal contact with the support plate. The actuator body is fixed to the opposite side of the support plate. The cooling means is disposed in thermal communication between the support plate and the actuator body. The cooling means is a structure that removes heat from the pump head and transfers the heat to the actuator body.

  In another aspect, the invention features an actuator having a thermally conductive member having an outer surface, a pump head having a chamber for flowing pressurized fluid, and cooling means for cooling the pump head. The cooling means is in thermal communication with the pump head inside. The cooling means is a structure that removes heat from the pump head and transfers the heat to a thermally conductive member having an outer surface.

  In another aspect, the invention features a method for cooling a pump head of an actuator. The method includes thermally contacting the pump head and the thermally conductive support plate, thermally contacting the cooling means and the support plate, and thermally coupling the cooling means and the actuator body. Contacting and electrically controlling the cooling means to remove heat from the pump head and transfer it to the actuator body.

  In yet another aspect, the invention features a method for cooling a pump head of an actuator. The method includes the steps of thermally communicating a pump head and a cooling means inside the actuator, thermally communicating the cooling means and a thermally conductive member of the actuator having an outer surface, and transferring heat from the pump head. Electrically controlling the cooling means for removal and transmission to a thermally conductive member having an outer surface.

  The above and other advantages of the present invention will be better understood with reference to the following description and accompanying drawings. In the drawings, like reference numerals refer to like structural elements and features. The drawings are not necessarily to scale, emphasis instead being placed upon illustrating the principles of the invention.

FIG. 6 is a cross-sectional view of an embodiment of an actuator having a structure with an internal cooling module for cooling a pump head. It is an enlarged view of an actuator. It is sectional drawing of the actuator of the structure which has one Embodiment of an internal cooling module. It is a photograph of an actuator having a structure having an internal cooling module. It is a graph of the test result obtained by the internal cooling module. It is sectional drawing of the actuator of the structure which has one Embodiment of a prechiller unit. FIG. 7 is a diagram of a supercritical fluid chromatography system using the actuator shown in FIG. 6.

  A cooling module for independently controlling the temperature of the pump head described herein is installed within the actuator. In summary, the cooling module removes heat from the pump head and transfers it to an actuator member, mechanism, or component having an outer surface, preferably the thermally conductive actuator body itself. In one embodiment, the cooling module consists of a thermoelectric element inserted between two heat conducting plates. One of the heat conducting plates is in thermal communication with the pump head (eg, via a support plate) and the other of the heat conducting plates is in thermal communication with the actuator mechanism.

  Advantageously, the cooling module is not visible to the user, i.e. in some embodiments there are no new parts in an area accessible to the user of the actuator and the cooling module is located behind the support plate. Has been. From a maintenance point of view, there is no need to change pump head parts to install the cooling module in the actuator, so a new procedure to replace the pump head seal is not required. Among these advantages, the solid state components used to form the cooling module require no maintenance. In addition, the cooling module can improve the thermal stability of the pump head, improve density control regardless of ambient temperature, and achieve accurate mass flow under conditions where the pressure of the fluid is known.

  1 and 2 illustrate an embodiment of an actuator 10 having a pump head 12 and an actuator body 14. (FIG. 2 is an enlarged view of the actuator 10 near the pump head 12). The pump head 12 has one end fixed to the pressure transducer 16 and the other end fixed to one side of the support plate 18. Fixed to the opposite side of the support plate 18 is the actuator body 14. In one embodiment, the actuator 10 is part of a binary solvent manager (BSM) that uses two separate serial flow pumps to remove the solvent from the reservoir and deliver the solvent composition. An example implementation of BSM is the ACQUITY binary solvent manager from Waters (Milford, Mass.).

  The pump head 12 includes an outlet port 20, an inlet port 22, a fluid chamber 24, a hole opening 26, and a recess 28 that receives and aligns a housing 30 secured to the support plate 18. The fluid chambers 24 in the pump head 12 are in fluid communication with an outlet port 20 and an inlet port 22 for receiving and discharging fluid, respectively. In some embodiments, the housing 30 includes a chamber that collects liquid therein and cleans the plunger with any particulates that may adhere to the plunger surface. For example, seal assemblies such as low pressure seal assembly 32 and high pressure seal assembly 34 serve to contain liquid within housing 30.

  The actuator body 14 includes a motor 36 and a drive mechanism 38 mechanically coupled to the plunger 40. The plunger 40 extends through the hole opening 26 of the pump head 12 to the fluid chamber 24. Although the cooling mechanism described herein is shown connected to a reciprocating plunger, a rotating shaft such as, for example, a shaft that rotates to rotate a rotor attached to a stator. You may use the actuator which has. The term “rod” is used herein in a broad sense to include plungers, shafts, rods, and pistons, whether reciprocating or rotating. Reference numeral 42 corresponds to a compartment in the actuator body 14 and can be employed to accommodate a cooling module that controls the temperature of the pump head 12, as described in connection with FIG.

  FIG. 3 is a cross-sectional view of actuator 10 having a structure with one embodiment of internal cooling module 50 for independently controlling cooling of pump head 12. The cooling module 50 includes a thermoelectric element 52 disposed between the low temperature side plate 54 and the high temperature side plate 56. In one embodiment, the thermoelectric element 52 is a Peltier element and uses power to generate a temperature difference on both sides of the element by operating as a heat pump that transfers heat from one side to the other. The resulting temperature difference depends on several variables: the material properties of the thermoelectric element 52, the amount of heat removed from the cold side, the average temperature of the chamber, and the drive current / voltage. In this embodiment, the thermoelectric element has a central hole that accommodates the plunger 40. Other shapes of thermoelectric elements may be used as long as they do not interfere with the movement of the plunger.

  The low temperature side plate 54 is in thermal contact with the support plate 18. The material of the support plate 18 is selected so as to improve the thermal conductivity. The high temperature side plate 56 is in thermal contact with the actuator body 14. Other than the actuator body 14 or in addition to the actuator body 14, other heat conductive members, mechanisms, or components of the actuator may function as the high temperature side sink. Similarly, the low temperature side plate 54 and the high temperature side plate 56 have a central hole for accommodating the plunger 40. An electrode (not shown) for controlling the operation of the thermoelectric chip 52 extends between the insulator 58 and the high temperature side plate 56. In one embodiment, the hot side plate 56 is made of copper. An insulator 58 is disposed around the low temperature side plate 54 and the thermoelectric chip 52 to insulate the low temperature side plate 54 and the thermoelectric chip 52 from the ambient environment and minimize thermal communication between the high temperature surface and the low temperature surface. . The hot side plate 56 has an outer surface 60 so that heat is radiated directly from the hot side plate 56 to the surrounding environment. The fastener 62 fixes the cooling module 50 to the support plate 18. During operation of the cooling module, the low temperature side plate 54 extracts heat from the pump head 12 and transfers it to the high temperature side plate 56. Heat is transferred from the hot side plate 56 to the actuator body 14 and heat is radiated, conducted or convected from the actuator body 14 to the surrounding environment. A heat sink, fan, and / or liquid cooling device may be used on the hot side to cool the hot side.

  Temperature measurements may be made for feedback control at one or more positions within the actuator. In a preferred embodiment, a temperature sensor is located at or near the cold side plate 54.

  FIG. 4 is a photograph from two different angles of an actuator having a structure with an internal cooling module. The visible portions of the cooling module are the high temperature side plate 56 and the insulator 58.

  FIG. 5 is a graph of test results obtained by one embodiment of the internal cooling module. The x axis corresponds to the duty cycle in which the Peltier element 52 is operated. The y-axis is the amount of heat (watts) removed from the pump head and transferred from the cold side plate to the hot side plate. Each of the four plots shows one of four test combinations of Peltier element operating voltage (10 v or 12 v) and fan size (small or large). A red horizontal line indicates a preferable amount of heat to be removed. The four plots show that when the cooling module is operated at a 100% duty cycle, the amount of heat removed can have a margin of 20-50% over the preferred amount of heat removed.

  In another embodiment, a prechiller unit is disposed (eg, bolted) between the support plate 18 and the cold side plate 54 of the cooling module 50. FIG. 6 is a cross-sectional view of the actuator 10 having a structure having the prechiller unit 70. The prechiller unit 70 functions to cool the fluid before it enters the fluid chamber 24.

  The prechiller unit 70 includes a prechiller body 72 that is in thermal conductive contact with the support plate 18 and the low temperature side plate 54. The prechiller body 72 is made of a heat conductive material (for example, copper). The prechiller body 72 forms a through hole 74 that accommodates the plunger 40.

  Adding the prechiller unit 70 between the actuator body 14 and the pump head 12 increases the number of parts, resulting in a larger tolerance stackup. In order to overcome this problem, the length of the plunger 40 (proximal end 41 of the plunger 40) behind the low pressure seal assembly 32 may be extendable.

  Further, the prechiller unit 70 includes a fluid pipe 76 disposed in the recess 77 of the prechiller body 70 and in thermal communication with the prechiller body 70. The fluid piping 76 is held in the recess 77 by heat-resistant epoxy. Alternatively or additionally, thermal grease may be used in the recesses 77 to ensure heat transfer between the prechiller body 70 and the fluid piping 76. Alternatively, or in addition, solder may be used to hold the fluid piping 76 within the recess 77 and ensure thermal communication with the prechiller body 70. Alternatively, grooves may be machined in the copper plate. The fluid piping 76 includes five turns of 0.040 inner diameter stainless steel tube 78 that surrounds the through hole 74 and defines the fluid volume of the prechiller unit 70. The fluid volume of the prechiller unit 70 is preferably greater than the fluid volume of the fluid chamber 24 (ie, the volume that can receive fluid when the plunger 40 is located at the end of the suction stroke), eg, from about 140 μL. large. In this regard, the prechiller unit 70 can have a fluid volume of about 400 μL to about 500 μL, for example, about 426 μL. The fluid volume of the prechiller unit 70 can be greater than about three times the fluid volume of the fluid chamber 24. The fluid line 76 includes an inlet 80 and an outlet 82 that are connected to or integral with the tube 78, thereby allowing an external fluid connection.

  During operation, the low temperature side plate 54 extracts heat from the prechiller unit 70 and transfers it to the high temperature side plate 56. Heat is transferred from the hot side plate 56 to the actuator body 14 and heat is radiated, conducted or convected from the actuator body 14 to the surrounding environment. Similarly, the cooling of the prechiller unit 70 has an effect of cooling the pump head 12 by the heat conductive contact between the pump head 12 and the support plate 18 and the heat conductive contact between the support plate 18 and the prechiller unit 70.

  FIG. 7 is a diagram showing a supercritical fluid chromatography system 100 using the actuator 10 of FIG. The SFC system 100 includes a plurality of stackable modules including a solvent manager 110, an SFC manager 140, a sample manager 170, a column manager 180, and a detector module 190.

  The solvent manager 110 comprises a first pump 112 that receives CO2 from a carbon dioxide (CO2) source 102 (e.g., a tank containing compressed CO2). The CO 2 passes through the inlet shutoff valve 142 and the filter 144 of the SFC manager 140 on the way to the first pump 112. The first pump 112 includes an accumulator actuator 10a and a main actuator 10b connected in series. The accumulator actuator 10a sends CO2 to the system 100. The main actuator 10b replenishes the accumulator actuator 10a and sends CO2 to the system 100 while replenishing the accumulator actuator 10a.

  The accumulator actuator 10a and the main actuator 10b each have the structure shown in FIG. 6 and are designed to perform multi-stage precooling of CO2. The CO2 moves from the SFC manager 140 through the prechiller unit 70a of the accumulator actuator 10a. The accumulator actuator 10a is controlled to a temperature of about 12 ° C. by an internal cooling module. The CO 2 moves through the pre-chiller unit 70b of the main actuator 10b after passing through the pre-chiller unit 70a of the accumulator actuator 10a. The main actuator 10b is controlled to a temperature of about 2 ° C. by the internal cooling module.

  The CO 2 passes through both the prechiller units 70a, 70b at a relatively low pressure (eg, about 700 psi to about 1200 psi) before passing through the fluid chamber of the main actuator 10b (see, eg, item 24 in FIG. 6). Then, it passes through the fluid chamber of the accumulator actuator 10a.

  Since the accumulator actuator 10a is controlled at 12 ° C., CO2 is likely to be gaseous when passing through the prechiller unit 70a of the accumulator actuator 10a. In order to ensure that CO2 is sent in liquid form to the system 100, the liquefaction of CO2 is performed by the main actuator 10b. Since the fluid volume of the prechiller unit 70b is larger than the fluid volume of the fluid chamber of the main actuator (ie, the volume when the plunger reaches the end of the suction stroke), a sufficient volume of CO2 is reliably available, The main actuator 10b can liquefy CO2 before it passes through the pump head of the accumulator actuator 10a.

  The accumulator actuator 10a serves as a metering device that meters the flow of CO2 to the system 100. It may be particularly advantageous to be able to control the temperature of the accumulator actuator 10a (eg by an internal cooling module). More specifically, the mass flow rate depends on temperature as well as pressure and volume flow rate. Thus, the ability to control the temperature provides a more accurate mass flow rate and can provide more accurate chromatography.

  In some examples, the solvent manager 110 further includes a second pump 114. The second pump 114 can include a main actuator 116 and an accumulator actuator 118 connected in series to receive an organic co-solvent (eg, methanol, water (H 2 O), etc.) from the organic co-solvent source 104. The accumulator actuator 118 delivers the co-solvent to the system 100. The main actuator 116 delivers co-solvent to the system 100 while replenishing the accumulator actuator 118.

  In order to monitor the pressure, a transducer is connected to the outlet port of each pump head. The solvent manager 110 further includes an electric drive for driving the main and accumulator actuators of the first pump 112 and the second pump 114. The CO2 and organic co-solvent fluid streams are mixed at the tee 120 to form a mobile phase fluid stream that continues to the injection valve subsystem 150, which injects the sample plug for separation into the mobile phase fluid stream. Inject.

  In the illustrated example, the injection valve subsystem 150 comprises an auxiliary valve 152 disposed within the SFC manager 140 and an injection valve 154 disposed within the sample manager 170. The auxiliary valve 152 and the injection valve 152 are fluidly connected and the operation of these two valves is adjusted to introduce the sample plug into the mobile phase fluid flow. The injection valve 154 operates to extract a sample plug from a sample source (eg, a vial) within the sample manager 170, and the auxiliary valve 152 controls the flow of mobile phase fluid to and from the injection valve 154. To work. The SFC manager 140 further includes a valve actuator for actuating the auxiliary valve 152 and an electric drive for driving the actuation of the valve. Similarly, the sample manager 170 further includes a valve actuator that operates the injection valve 154 and an electric drive for driving the operation of the valve.

  The mobile phase stream containing the injected sample plug moves from the injection valve subsystem 150 into the separation column 182 in the column manager 180 where the sample plug is separated into individual components. The column manager 180 includes a plurality of separation columns and an inlet switching valve 184 and an outlet switching valve 186 for switching between various separation columns.

  The mobile phase fluid stream passes through the separation column 182 and then travels to a detector 192 (eg, a flow cell / photodiode array type detector) housed in the detector module 190, after which the exhaust valve 146. Through to the back pressure regulator 148 in the SFC manager 140 before being discarded into the waste bin 106. A transducer 149 is disposed between the discharge valve 146 and the back pressure regulator 148.

  The back pressure regulator 148 can be adjusted to control or change the fluid pressure of the system. Thus, the pressure can be changed every time the system is operated. The nature of CO2 affects the rate at which compounds are extracted from the separation column 182, so that the pressure can be changed to enable different separations based on pressure. Typically, the back pressure regulator 148 is used to maintain the system pressure in the range of about 1500 psi to about 6000 psi.

  Further, as schematically shown in FIG. 7, a computer-based system control device 108 is shown, which can support the adjustment operation of the SFC system 100. Each of the individual modules 110, 140, 170, 180, 190 further includes its own control electronics and can interface with each other and with the system controller 108 via an Ethernet connection 109. The control electronics of each module are computer readable instructions (firmware) for controlling the operation of the components (eg, pumps, valves, etc.) of each module in response to signals received from the system controller 108 or other modules. ) May be included. The control electronics of each module may further include at least one processor for executing computer readable instructions, receiving inputs and transmitting outputs. The control electronics further 1 converts the digital output from one of the processors into an analog signal for operating an associated pump or valve of the pump or valve (eg, by an actuator of the associated pump or valve). One or more digital / analog (D / A) converters may be included. The control electronics further includes, for example, one or more analog / digital (A / D) converters for converting an analog signal from a system sensor (eg, pressure transducer) into a digital signal that is input to one of the processors. May be included. In some examples, some or all of the various mechanisms of these control electronics may be incorporated into the microcontroller.

  While one embodiment has been described in which a chiller is used to cool the fluid before it enters the fluid chamber of the pump head, in another embodiment, a pre-cooler that cools the fluid after it exits the pump head has been described. A chiller unit may be used.

  Although the invention has been illustrated and described with respect to certain preferred embodiments, it should be understood that those skilled in the art will recognize that the embodiments and forms of these embodiments may be practiced without departing from the spirit and scope of the invention as defined by the following claims. It will be understood that the details may be changed in various ways. For example, although the specification has primarily described reciprocating plunger applications, various embodiments of the cooling system can also be used in rotary plunger applications. Further, if necessary, other heat removal means may be used with the cooling modules described herein to remove larger loads. Also, although described with respect to SFC applications, the principles of the present invention may be implemented in actuators used in any other type of application where pump head temperature control is desirable. For example, pump head temperature control provides more reproducible and accurate results for other types of liquid chromatography applications such as HPLC and UPLC, regardless of ambient temperature.

Claims (9)

A support plate;
A pump head fixed to one side of the support plate and in thermal contact with the support plate , comprising an outlet port, an inlet port, a fluid chamber extending between the outlet port and the inlet port, and a hole opening A pump head comprising:
Is secured to the opposite side of the support plate from the pump head, an actuator body,
A plunger extending through the hole opening in the pump head to the fluid chamber, the plunger being displaceable between a first delivery end at a stroke position and a second suction end at a stroke position;
A pre-chiller unit comprising a pre-chiller body and fluid piping in thermal communication with the pre-chiller body, wherein the pre-chiller body is thermally coupled to the support plate to cool the fluid stream before it enters the pump head. The prechiller unit in communication,
An actuator comprising :
An actuator wherein the fluid volume of the fluid piping is greater than the fluid volume of the fluid chamber when the plunger is at the suction end of the stroke position . The actuator according to claim 1 , wherein the pre-chiller unit is disposed between the support plate and the actuator body. The actuator of claim 1 , wherein the fluid volume of the fluid piping is at least twice as large as the fluid volume of the fluid chamber when the plunger is at the suction end of the stroke position. The actuator of claim 1 , wherein the fluid volume of the fluid piping is at least three times greater than the fluid volume of the fluid chamber when the plunger is at the suction end of the stroke position. The actuator of claim 1 , wherein the prechiller body defines a recess and the fluid piping is disposed within the recess. The actuator according to claim 1 , wherein the prechiller unit main body is made of copper and the fluid piping is made of stainless steel . The actuator of claim 1 , further comprising a cooling module disposed to cool the prechiller unit, wherein the prechiller unit is disposed in thermal communication between the support plate and the cooling module. The cooling means includes a set of heat conducting plates, one of which is in thermal communication with the prechiller unit and the other in thermal communication with the actuator body, and a heat conducting plate and a heat between the set of heat conducting plates. A thermoelectric element that is in conductive contact and has a structure for transferring heat from a heat conduction plate that is in thermal communication with the prechiller unit to the other heat conduction plate that is in thermal communication with the actuator body. The actuator according to claim 7 , comprising a thermoelectric element. The actuator according to claim 7 , wherein the cooling module has a structure for cooling the pump head by thermally connecting the cooling module, the prechiller unit, the support plate, and the pump head.

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